The contents of copper, iron, lead, cadmium, cobalt and nickel in baking powder and baking soda samples have been determined by atomic absorption spectrometry after separation and preconcentration. Two different separation/preconcentration methods including APDC-Chromosorb 102 solid phase extraction method and Ce(OH)(4) coprecipitation method have been used for this purpose. The effects of main components of the baking soda and powder were examined. The methods were successfully applied for the determinations of Cu, Fe, Pb, Cd, Co and Ni in the baking soda and baking powder samples purchased from the local markets in Kayseri City-Turkey (recoveries greater than 95%). The results found the two preconcentration methods generally agree with each other. The levels of the analytes in the samples were below the allowed limit values given by Turkish Authorities.